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This review covers the investigations carried out with my colleagues and students during the last 25 years aimed at the development of analytical procedures for the preconcentration and/or speciation analysis of trace and ultra-trace elements using bio- and nanosorbents employing different methodologies, analytical techniques, and instrumental approaches. In the last years, an important part of this research was based on the use of nanomaterials for preconcentration and/or speciation studies. For their properties, they constitute a break